HRID1086955
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution consisting of 3.2 g of 5-amino-6-fluoro-3-propargyl-2-benzothiazolone and 50 g of dioxane were dropwise added 2.4 g of trichloromethyl chlorocarbonate at a temperature in the range of from 5° to 15° C. and the resulting mixture was heated under reflux for six hours. A residue was obtained by distilling off the low-boiling material from the mixture under reduced pressure, and it was dissolved in 150 ml of dried toluene and filtered. From the resulting filtrate toluene was distilled off to obtain 3.6 g of 6-fluoro-5-isocyanato-3-propargyl-2-benzothiazolone having a melting point in the range from 134° to 135° C.
WORKUP
后处理
- customof from 5° to 15° C.
- temperaturethe resulting mixture was heated
- temperatureunder reflux for six hours
- customA residue was obtained
- distillationby distilling off the low-boiling material from the mixture under reduced pressure, and it
- dissolutionwas dissolved in 150 ml of dried toluene
- filtrationfiltered
- distillationFrom the resulting filtrate toluene was distilled off